CN115635620A - Preparation method of high-uniformity ultrathin waterborne polyurethane condom - Google Patents
Preparation method of high-uniformity ultrathin waterborne polyurethane condom Download PDFInfo
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Abstract
The invention belongs to the technical field of contraception production, and particularly relates to a preparation method of a high-uniformity ultrathin aqueous polyurethane condom. The method comprises the following steps: preparing aqueous polyurethane emulsion, wherein the solid content of the aqueous polyurethane is 15-30%; dipping the isolating layer emulsion; soaking the treated mould into the waterborne polyurethane emulsion, drying, repeating for 2-3 times, and obtaining a waterborne polyurethane adhesive film on the surface of the mould; then carrying out operations such as curling, baking, demoulding and the like to obtain the waterborne polyurethane condom product. The method is simple, safe and easy to control; ultrathin aqueous polyurethane condoms of the 001 and 002 series are obtained. The prepared condom has the advantages of ultrathin thickness, uniform thickness distribution, no allergy, high strength, good flexibility and the like.
Description
Technical Field
The invention belongs to the technical field of contraception production, and particularly relates to a preparation method of a water-based polyurethane condom.
Background
The condom is also called condom, it is one of the simple ways of stopping pregnancy in non-medicine form, and it also has the function of preventing the transmission of venereal diseases such as gonorrhea and AIDS. The condom raw material is usually natural latex which contains components such as allergic water-soluble protein, and although the natural latex used for preparing the condom is subjected to deproteinization treatment, a small amount of the allergic water-soluble protein still exists, and about 8% of people are allergic to the latex.
The water-based polyurethane material has good biocompatibility, and compared with natural latex condoms, condoms made of water-based polyurethane have the advantages of no toxicity, high toughness and strength, good thermal conductivity and the like, can be made to be 0.01 to 0.03mm in ultrathin thickness, reduce the estrangement sense during use, increase the pleasure of users, have more compact structures, and have better barrier property on sperms, AIDS viruses, hepatitis B viruses and the like.
Because the molecular chain structure of the waterborne polyurethane material has more polar groups and stronger polarity, when materials with stronger polarity such as glass molds and the like are used as production molds, the adhesion force of the formed products on the mold surface is higher, the demolding is inconvenient, particularly, the demolding on an industrial production line is difficult, the integrity of the product adhesive film is often damaged or the product adhesive film generates permanent deformation, and the product percent of pass is generally only about 70-80%.
The average thickness of the adhesive film of a general product of the commercially available polyurethane condom is about 0.019-0.028mm, the thickness of the adhesive film gradually increases from the thinnest curled edge of the opening end to the seminal vesicle storage part at the closed end, referring to the HT/T5456-2018 or GB/T7544 idt ISO4074 standard thickness test method, the thickness of the adhesive film at the position close to the 35mm of the opening end is about 10-20% thicker than that at the position close to the 35mm of the opening end, a part of a user with the thicker adhesive film feels relatively obvious, the comfort of the user is affected, the typical example is that the thickness of the adhesive film at the position close to the 35mm of the opening end is 26mm, and the thickness of the adhesive film at the position 35mm of the opening end is 21mm.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a high-uniformity ultrathin aqueous polyurethane condom.
The invention provides a preparation method of a high-uniformity ultrathin waterborne polyurethane condom, which comprises the following specific steps:
s1: preparing the aqueous polyurethane emulsion to have a solid content of 15-30% and a viscosity of 15-30mPa.S;
s2: cleaning a mould: cleaning the glass mold with special cleaning solution, rinsing with deionized water, and drying, wherein the cleaning solution comprises but is not limited to 2-10% of white liquor, 1-8% of dilute acid solution, and 1-10% of neutral cleaning solution;
s3: dipping the isolated layer emulsion: immersing the mould into the separant emulsion for 3-10 seconds, slowly taking out the mould at the lifting speed of 2.0-3.0mm/s, and drying at 65-100 ℃ for 2-6min;
the isolation layer emulsion is a compound modified aqueous polyurethane emulsion with the solid content of 3-8%, and is prepared by compounding an organic silicon modified aqueous polyurethane emulsion, a nano silicon dioxide modified polyether aqueous polyurethane emulsion, a wetting agent, a flatting agent and a defoaming agent and filtering the mixture through a 400-mesh filter screen;
s4: dipping and film forming: immersing the mould processed in the step S3 into the aqueous polyurethane emulsion prepared in the step S1 under the condition that the relative humidity is more than 80%, wherein the immersion time is 3-10 seconds, the mould is slowly taken out at the lifting speed of 2.0-3.0mm/S, then drying for 3-8min at the temperature of 65-110 ℃, and repeating the step S4 for 2-4 times to obtain an aqueous polyurethane adhesive film on the surface of the mould;
s5: edge curling: carrying out edge curling treatment on the opening end of the waterborne polyurethane adhesive film on the surface of the die;
s6: baking: putting the mould processed in the step S5 into an oven, and baking at 70-120 ℃ for 15-30 min;
s7: dipping a release agent: immersing the mould treated in the step S6 into a special isolation release agent with the solid content of 1-8%, taking out and drying for 6-15min at the temperature of 80-110 ℃;
s8: demoulding: demolding the mold treated in the step S7 by adopting a brush roller or a rubber roller to obtain a semi-product of the waterborne polyurethane condom;
s9: electric detection: and (5) performing high-voltage dry electrical inspection on the semi-finished product of the waterborne polyurethane condom obtained in the step (S8) and removing defective products to obtain a qualified waterborne polyurethane condom product.
Preferably, the aqueous polyurethane emulsion in the step S1 is a polyether/polyester type aqueous polyurethane emulsion having high strength, low modulus and high resilience, and more preferably, 100% young' S modulus is 0.9 to 1.3MPa, tensile strength is 45MPa or more, and permanent set is within 5%.
Preferably, the cleaning solution in the step S2 includes, but is not limited to, 2-10% of white liquor, 1-8% of diluted acid solution, and 1-10% of neutral cleaning solution.
Preferably, the wetting agent and the leveling agent adopted in the isolation layer emulsion in the step S3 are polyether modified polysiloxane polymers, and the defoaming agent is a polyether modified polysiloxane solution, with an addition amount of 0.05-0.2%.
Preferably, the special isolating and releasing agent in the step S7 is one or two of a white carbon black aqueous dispersion, a modified corn starch aqueous dispersion, an ultrafine calcium carbonate aqueous dispersion and a cellulose aqueous dispersion.
Preferably, the water-based polyurethane condom product qualified by electric inspection is added with a lubricant for heat sealing and packaging, and the added lubricant is silicone oil or a water-based lubricant, preferably ultra-smooth silicone oil or a hyaluronic acid water-based lubricant.
In the invention, the average thickness drop between the 35mm position of the closed end and the 35mm position of the open end of the condom is not more than 6.5 percent, thereby meeting the requirement of high uniformity.
The modified waterborne polyurethane emulsion used as the isolation layer emulsion has the following advantages:
(1) Due to the polarity of molecular chain groups of the waterborne polyurethane material, when a non-polar or weakly polar material is used as a mold for dipping and film forming, such as polypropylene (PP), polyethylene terephthalate (PET), polytetrafluoroethylene and the like, the hydrophobicity of the surface of the mold is higher, the spreading and film forming property of emulsion on the surface of the mold is poor, the uniformity of a glue film is poor, and the qualification rate of a product is reduced, while when the mold made of stainless steel, glass and the like is used, the bonding force between the polyurethane glue film and the surface of the mold is stronger, so that the formed product is difficult to demould;
(2) According to the preparation method of the high-uniformity ultrathin waterborne polyurethane condom, the solid content and the viscosity characteristic of the emulsion are properly matched with the lifting speed (2.0-3.0 mm/s) of the mould after dipping, and the lifting speed of the mould during specific production is determined according to the following formula:
V=C*δ/（∑TS i *μ i ) Wherein i is 1,2,3 or 1,2,3,4;
v- - -lifting speed, m/s;
c- -specific relation constant related to emulsion and mould characteristics, and the value is 9.725 x10 by test verification 3 ；
Delta-single layer thickness of the product, mm;
TS- - -total solid content of the glue tank polyurethane emulsion,%;
mu- - -viscosity of the polyurethane emulsion in the glue groove, mPa.S;
the thickness distribution of the glue film of the product of the ultrathin water-based polyurethane condom formed by dipping is very uniform, when the test is carried out by adopting a 3-point method of a HT/T5456-2018 or GB/T7544 idt ISO4074 standard thickness test method, the difference between the average glue film thickness at 35mm at the closed end and 35mm at the open end is not more than 6.5%, and under the stable condition, the difference between the average glue film thickness at the typical value is not more than 3.5%.
The method is simple, safe and easy to control. The 001 and 002 series high-uniformity ultrathin waterborne polyurethane condoms can be obtained by the method, and the method has the advantages of ultrathin polyurethane condoms, safety, no allergy, good heat conductivity and the like, and particularly has the advantages of uniform film thickness distribution, high tearing strength, good flexibility (low modulus), high yield and the like. Typical product performance data compared to commercial samples are as follows:
the test method of the main performance of the product is as follows:
(1) Testing the tensile property by using a universal tensile testing machine according to the method of GB/T528-2009, wherein the sample is a dumbbell-shaped sheet, the tensile rate is 300 mm/min, and the temperature is 25 ℃;
(2) And (3) testing the tearing strength: testing by using a universal tensile testing machine according to the method of GB/T528-2009, wherein the sample is a right-angle test sample, the tensile rate is 500 +/-50 mm/min, and the temperature is 25 ℃;
(3) And (3) testing puncture strength: according to the GB/T10004-2008 standard test, a sample membrane is cut into strip-shaped blocks by using scissors, wherein the width of the strip-shaped film is required to be more than 100X100mm; mounting a test piece with the width of 100mm on a sample membrane fixing clamp ring, then removing top pricks by using a steel needle with the diameter of 1.0mm and the radius of the top end of the diameter of 0.1mm at the speed of (50 +/-5) mm/min, and reading the heavy load of the steel needle penetrating the test piece; testing 3 points, and taking the arithmetic mean value;
(4) The thickness of the adhesive film is measured by a thickness meter method (Shanghai Heizi instruments factory) of appendix F in GB/T7544-2019 standard;
5. the viscosity is measured at 25 ℃ with a rotational viscometer type NDJ-1;
(5) The blasting performance of the product is tested by adopting the method of annex H in the HT/T5456-2018 standard.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1
S1: blending the water-based polyurethane emulsion for condoms:
adding deionized water into the waterborne polyurethane emulsion under the stirring state, diluting until the solid content is 18.5%, and stirring for 20 minutes; filtering the diluted emulsion through 400-mesh filter cloth, and respectively placing the filtered emulsion into a first emulsion impregnation tank, a second emulsion impregnation tank and a third emulsion impregnation tank for standing for 24 hours for later use; the emulsion viscosity was measured with a rotational viscometer to be 140mpa.s; the waterborne polyurethane emulsion is polyether/polyester waterborne polyurethane emulsion with high strength, low modulus and high resilience;
s2: cleaning a mold:
the mold is a glass mold and is fixed on a clamp, under the production condition, a soft brush and a neutral detergent are used for cleaning the mold at normal temperature, the soft brush and deionized water are used for cleaning the mold at normal temperature, finally ultrapure water (the conductivity is 0.1-0.2 us/cm) at (50 +/-5) DEG C is used for cleaning the mold, and the mold is dried in an oven at the drying temperature of 75-80 ℃ for 2-3 minutes;
s3: emulsion for dipping isolation layer
Cooling the dried mould in the step S2 to 38-40 ℃ through a constant-temperature air duct, immersing the mould into the isolation layer emulsion for 3-5 seconds, slowly taking out the mould at the lifting speed of 2.0mm/S, and drying the mould in an oven after the mould surface is discharged, wherein the drying temperature is 65-70 ℃ and the drying time is 5-6 minutes;
s4: dipping and film forming:
cooling the mould processed in the step S3 to 38-40 ℃ through a constant temperature air duct, immersing the mould in an emulsion dipping tank for 3-5 seconds, slowly taking out the mould at the lifting speed of 2.0mm/S, taking out the mould, humidifying and spraying the mould for 20 seconds, and then drying the mould in an oven at the drying temperature of 65-70 ℃ for 7-8 minutes;
this is a dip, this step is repeated 3 times;
s5: edge curling:
forming a waterborne polyurethane adhesive film on the surface of the die after the treatment of the step S4, and performing edge curling treatment on the opening end of the adhesive film on the surface of the die by using a rubber roller, wherein the total length after edge curling is more than or equal to 180 mm;
s6: baking: placing the mould processed in the step S5 into an oven for baking, wherein the drying temperature is set to be 110-120 ℃, and the drying time is 15-18 minutes;
s7: dipping a release agent: immersing the mould treated in the step S6 into a special isolation release agent (nano silicon dioxide) with the solid content of 3 percent, taking out and drying for 13-15 min at the temperature of 80-85 ℃;
s8: demoulding: demolding the mold treated in the step S7 by adopting a brush roller or a rubber roller to obtain a semi-product of the waterborne polyurethane condom;
s9: electric detection: and (5) performing high-voltage dry electrical inspection on the semi-finished product of the waterborne polyurethane condom obtained in the step (S8), and removing defective products to obtain a qualified waterborne polyurethane condom product.
The selected aqueous polyurethane emulsion is polyether/polyester type aqueous polyurethane emulsion with high strength, low modulus and high resilience, and the 100 percent Young modulus of the emulsion is 1.2MPa, the tensile strength is 48.3MPa, and the permanent deformation is 2.2 percent.
Preparing an isolation layer emulsion: the isolation layer emulsion is a compound modified waterborne polyurethane emulsion with the solid content of 5%,10 kg of nano silicon dioxide modified polyether waterborne polyurethane emulsion with the solid content of 25% and 5kg of 50% organic silicon copolymerization modified waterborne polyurethane emulsion are added into 84.6kg of deionized water, 0.15kg of wetting agent, 0.15kg of flatting agent and 0.1kg of defoaming agent are added into the deionized water, and then the mixture is stirred to be uniform and then filtered by a 400-mesh filter screen.
Preparing a release agent: after adding 3kg of white carbon black (nano silicon dioxide) and 0.5kg of water-based wetting agent into 96.3kg of deionized water, adding 0.2kg of surfactant and stirring uniformly. The purpose of adding the water-based wetting agent is to improve the sagging uniformity of the white carbon black on the surface of the adhesive film, and the water-based wetting agent can be a polyether modified organic silicon wetting agent.
The thickness of the polyurethane condom obtained in the embodiment is 0.016mm, the tensile strength is 50.15Mpa, the breaking elongation is 1068%, the 100% definite modulus is 1.19Mpa, the 300% definite modulus is 2.41Mpa, and the qualification rate of a semi-finished product after high-voltage electrical inspection is 93.2%.
Example 2
S1: preparing the aqueous polyurethane emulsion for condoms:
adding deionized water into the waterborne polyurethane emulsion under the stirring state, diluting until the solid content is 20.5%, and stirring for 20 minutes; filtering the diluted emulsion through 400-mesh filter cloth, and respectively placing the filtered emulsion into a first emulsion impregnation tank, a second emulsion impregnation tank and a third emulsion impregnation tank for standing for 24 hours for later use; the emulsion viscosity was measured with a rotational viscometer to be 140mpa.s; the aqueous polyurethane emulsion is polyether/polyester type aqueous polyurethane emulsion with high strength, low modulus and high resilience;
s2: cleaning a mould:
the mold is a glass mold and is fixed on a clamp, under the production condition, a soft brush and 2-5% alkali liquor are used for cleaning the mold at normal temperature, then the soft brush and deionized water are used for cleaning the mold at normal temperature, finally ultrapure water (the conductivity is 0.1-0.2 us/cm) at (55 +/-5) DEG C is used for cleaning the mold, then the mold enters an oven for drying, the drying temperature is 80-85 ℃, and the drying time is 2-3 minutes;
s3: separant tank impregnation
Cooling the mould dried in the step S2 to 43-45 ℃ through a constant temperature air duct, immersing the mould into a separant, and drying the mould in an oven after the mould comes out of liquid, wherein the drying temperature is 75-80 ℃ and the drying time is 4-5 minutes;
s4: dipping and film forming:
cooling the mould processed in the step S3 to 45 ℃ through a constant-temperature air duct, immersing the mould into a first emulsion dipping tank for 3-5 seconds, slowly taking out the mould at the lifting speed of 2.07mm/S, taking out the mould, humidifying and spraying the mould for 20 seconds, and then drying the mould in an oven at the drying temperature of 75-80 ℃ for 5-6 minutes;
this is a dip, this step is repeated 3 times;
s5: edge curling:
forming a waterborne polyurethane adhesive film on the surface of the die after the treatment of the step S4, and curling the opening end of the adhesive film on the surface of the die by using a rubber roller, wherein the total length after curling is more than or equal to 185 mm;
s6: baking: placing the mould processed in the step S5 into an oven for baking, wherein the drying temperature is set to be 85-95 ℃, and the drying time is 22-25 minutes;
s7: dipping a release agent: immersing the mould processed in the step S6 into a special isolation release agent (superfine calcium carbonate) with the solid content of 2.5 percent, taking out and drying for 10-12 min at the temperature of 90-95 ℃;
s8: demoulding: demolding the mold treated in the step S7 by adopting a brush roller or a rubber roller to obtain a semi-product of the waterborne polyurethane condom;
s9: electric detection: and (5) performing high-voltage dry-method electrical inspection on the semi-finished product of the waterborne polyurethane condom obtained in the step (S8) at 1600V, and removing defective products to obtain a qualified waterborne polyurethane condom product.
The selected aqueous polyurethane emulsion is polyether/polyester type aqueous polyurethane emulsion with high strength, low modulus and high resilience, and the 100 percent Young modulus of the emulsion is 1.2MPa, the tensile strength is 52.6MPa, and the permanent deformation is 2.1 percent.
Preparing an isolation layer emulsion: the isolation layer emulsion is a compound modified waterborne polyurethane emulsion with the solid content of 6%,10 kg of nano silicon dioxide modified polyether waterborne polyurethane emulsion with the solid content of 30% and 7.5kg of organic silicon graft modified waterborne polyurethane emulsion with the solid content of 40% are added into 82.1kg of deionized water, 0.18kg of wetting agent, 0.12kg of flatting agent and 0.1kg of defoaming agent are added into the deionized water, and then the mixture is stirred to be uniform and filtered by a 400-mesh filter screen.
Preparing a release agent: adding 2.5kg of superfine light calcium carbonate, 0.5kg of superfine light magnesium carbonate and 0.1kg aqueous wetting agent into 96.75kg of deionized water, adding 0.15kg of surfactant, and stirring uniformly. The purpose of adding the water-based wetting agent is to improve the sagging uniformity of the superfine light calcium carbonate on the surface of the adhesive film, and the water-based wetting agent can be polyether modified organic silicon wetting agent.
The thickness of the polyurethane condom obtained in the embodiment is 0.0194mm, the tensile strength is 52.06Mpa, the elongation at break is 1178%, the 100% definite elongation modulus is 1.16Mpa, the 300% definite elongation modulus is 2.31Mpa, and the qualification rate of the semi-finished product after high-voltage electric detection is 94.5%.
Example 3
S1: preparing the aqueous polyurethane emulsion for condoms:
adding deionized water into the waterborne polyurethane emulsion under the stirring state, diluting until the solid content is 19.0%, and stirring for 20 minutes; filtering the diluted emulsion through 400-mesh filter cloth, and respectively placing the filtered emulsion into a first emulsion impregnation tank, a second emulsion impregnation tank and a third emulsion impregnation tank for standing for 24 hours for later use; the emulsion viscosity was determined to be 143mpa.s with a rotational viscometer; the waterborne polyurethane emulsion is polyether/polyester waterborne polyurethane emulsion with high strength, low modulus and high resilience;
s2: cleaning a mold:
the mold is a glass mold and is fixed on a clamp, under the production condition, a soft brush and 1-3% alkali liquor are used for cleaning the mold at normal temperature, then the soft brush and deionized water are used for cleaning the mold at normal temperature, finally ultrapure water (the conductivity is 0.1-0.2 us/cm) at (60 +/-5) DEG C is used for cleaning the mold, then the mold is dried in an oven, the drying temperature is 85-90 ℃, and the drying time is 1-2 minutes;
s3: separant tank impregnation
Cooling the mould dried in the step S2 to 35-37 ℃ through a constant temperature air duct, immersing the mould into a separant, and drying the mould in an oven after the mould comes out of liquid, wherein the drying temperature is 85-90 ℃ and the drying time is 3-4 minutes;
s4: dipping and film forming:
cooling the mould processed in the step S3 to 35-37 ℃ through a constant temperature air duct, immersing the mould into a first emulsion dipping tank, wherein the dipping time is 4-6 seconds, slowly taking out the mould at a lifting speed of 2.75mm/S, taking out the mould, humidifying and spraying the mould for 15 seconds, and then drying the mould in an oven, wherein the drying temperature is 85-90 ℃, and the drying time is 3.5-4.5 minutes;
this is a dip, this step is repeated 3 times;
s5: edge curling:
forming a waterborne polyurethane adhesive film on the surface of the die after the treatment of the step S4, and curling the opening end of the adhesive film on the surface of the die by using a rubber roller, wherein the total length after curling is more than or equal to 185 mm;
s6: baking: placing the mould processed in the step S5 into an oven for baking, wherein the drying temperature is set to be 70-80 ℃, and the drying time is 25-30 minutes;
s7: dipping a release agent: immersing the mould processed in the step S6 into a special isolation release agent (modified corn starch isolation agent) with the solid content of 5.0 percent, taking out and drying for 8-10 min at the temperature of 95-100 ℃;
s8: demoulding: demolding the mold treated in the step S7 by adopting a brush roller or a rubber roller to obtain a semi-product of the waterborne polyurethane condom;
s9: electric detection: and (5) performing high-voltage dry-method electrical inspection on the semi-finished product of the waterborne polyurethane condom obtained in the step (S8) at 1600V, and removing defective products to obtain a qualified waterborne polyurethane condom product.
The selected aqueous polyurethane emulsion is polyether/polyester type aqueous polyurethane emulsion with high strength, low modulus and high resilience, and the 100 percent Young modulus of the emulsion is 1.08MPa, the tensile strength is 52.8MPa, and the permanent deformation is 2.8 percent.
Preparing an isolation layer emulsion: the isolation layer emulsion is a compound modified aqueous polyurethane emulsion with the solid content of 3%, 5kg of nano silicon dioxide modified polyether aqueous polyurethane emulsion with the solid content of 30% and 3.75kg of organic silicon graft modified aqueous polyurethane emulsion with the solid content of 40% are added into 90.9kg of deionized water, 0.15kg of wetting agent, 0.10kg of flatting agent and 0.1kg of defoaming agent are added into the deionized water, and then the mixture is stirred to be uniform and then filtered by a 400-mesh filter screen.
Preparing a release agent: 5% of modified corn starch separant is adopted. Adding 4.5kg of superfine modified corn starch, 0.5kg of superfine light magnesium carbonate and 0.15kg of kg aqueous wetting agent into 94.7 kg deionized water, adding 0.15kg of surfactant, and stirring uniformly. The purpose of adding the water-based wetting agent is to improve the sagging uniformity of the superfine light calcium carbonate on the surface of the adhesive film, and the water-based wetting agent can be a polyether modified organic silicon wetting agent.
The thickness of the obtained polyurethane condom is 0.023mm, the tensile strength is 53.93Mpa, the elongation at break is 1256%, the 100% definite modulus is 1.05Mpa, the 300% definite modulus is 2.09Mpa, and the qualification rate of the semi-finished product after high-voltage electric detection is 95.1%.
Example 4
S1: preparing the aqueous polyurethane emulsion for condoms:
adding deionized water into the waterborne polyurethane emulsion under the stirring state, diluting until the solid content is 22.0%, and stirring for 20 minutes; filtering the diluted emulsion through 400-mesh filter cloth, and respectively placing the filtered emulsion into a first emulsion impregnation tank, a second emulsion impregnation tank and a third emulsion impregnation tank for standing for 24 hours for later use; the emulsion viscosity was measured to be 1699 mPa.S with a rotational viscometer; the aqueous polyurethane emulsion is polyether/polyester type aqueous polyurethane emulsion with high strength, low modulus and high resilience;
s2: cleaning a mold:
the mold is a glass mold and is fixed on a clamp, under the production condition, a soft brush and 1-3% alkali liquor are used for cleaning the mold at normal temperature, then the soft brush and deionized water are used for cleaning the mold at normal temperature, finally ultrapure water (the conductivity is 0.1-0.2 us/cm) at (65 +/-5) DEG C is used for cleaning the mold, then the mold enters an oven for drying, the drying temperature is 90-95 ℃, and the drying time is 1-2 minutes;
s3: separant tank impregnation
Cooling the mould dried in the step S2 to 35-37 ℃ through a constant temperature air duct, immersing the mould into a separant, and drying the mould in an oven after the mould comes out of liquid, wherein the drying temperature is 95-100 ℃ and the drying time is 2-3 minutes;
s4: dipping and film forming:
cooling the mould processed in the step S3 to 48-50 ℃ through a constant temperature air duct, immersing the mould into a first emulsion dipping tank, wherein the dipping time is 3-5 seconds, slowly taking out the mould at a lifting speed of 3.0mm/S, taking out the mould, humidifying and spraying the mould for 20 seconds, and then drying the mould in an oven, wherein the drying temperature is 95-100 ℃, and the drying time is 3-4 minutes;
this is a dip, this step is repeated 2 times;
s5: edge curling:
forming a waterborne polyurethane adhesive film on the surface of the die after the treatment of the step S4, and curling the opening end of the adhesive film on the surface of the die by using a rubber roller, wherein the total length after curling is more than or equal to 185 mm;
s6: baking: placing the mould processed in the step S5 into an oven for baking, wherein the drying temperature is set to be 95-105 ℃, and the drying time is 22-25 minutes;
s7: dipping a release agent: immersing the mould treated in the step S6 into a special isolation release agent (superfine calcium carbonate) with the solid content of 2.5 percent, taking out and drying for 6-8 min at the temperature of 105-110 ℃;
s8: demoulding: demolding the mold treated in the step S7 by adopting a brush roller or a rubber roller to obtain a semi-product of the waterborne polyurethane condom;
s9: electric detection: and (5) performing high-voltage dry-method electrical inspection at 1650V on the semi-finished product of the waterborne polyurethane condom obtained in the step (S8), and removing defective products to obtain a qualified waterborne polyurethane condom product.
The aqueous polyurethane emulsion is polyether/polyester type aqueous polyurethane emulsion with high strength, low modulus and high resilience, and the 100 percent Young modulus of the aqueous polyurethane emulsion is 1.25MPa, the tensile strength is 55.8MPa, and the permanent deformation is 2.5 percent.
Preparing an isolation layer emulsion: the isolation layer emulsion is a compound modified aqueous polyurethane emulsion with the solid content of 8 percent, 15kg of nano silicon dioxide modified polyether aqueous polyurethane emulsion with the solid content of 30 percent and 8.75kg of 40 percent organic silicon graft modified aqueous polyurethane emulsion are added into 75.88kg of deionized water, 0.15kg of wetting agent, 0.12kg of flatting agent and 0.1kg of defoaming agent are added into the deionized water, and then the mixture is stirred to be uniform and filtered by a 400-mesh filter screen.
Preparing a release agent: 8 percent of special separant suspension is adopted, and the special separant suspension is prepared from white carbon black and hydroxyethyl cellulose powder 1:3. Adding 4.5kg of superfine modified corn starch, 0.5kg of superfine light magnesium carbonate and 0.15kg of kg aqueous wetting agent into 94.7 kg deionized water, adding 0.15kg of surfactant, and stirring uniformly. The water-based wetting agent is added to improve the sagging uniformity of the separant on the surface of the adhesive film, and the water-based wetting agent can be polyether modified organic silicon wetting agent.
The thickness of the obtained polyurethane condom is 0.023mm, the tensile strength is 57.23Mpa, the elongation at break is 1329%, the 100% modulus at definite elongation is 1.22Mpa, the 300% modulus at definite elongation is 2.39Mpa, and the qualification rate of the semi-finished product after high-voltage electric detection is 93.7%.
Further embodiments:
under the similar conditions of the example 4, the emulsion of the 1 st and 2 nd dipping is replaced, the emulsion with the total solid content of 28 percent and the viscosity of 173mPa.S is used, the lifting speed after dipping the emulsion is 2.6mm/s, the thickness of the polyurethane condom is 0.026mm, the tensile strength is 58.67Mpa, the elongation at break is 1365 percent, the 100 percent modulus of definite elongation is 1.25Mpa, and the 300 percent modulus of definite elongation is 2.42Mpa.
The relevant main process and product performance data of the examples are as follows:
the above data of the exemplary embodiment can be seen to have excellent thickness profile characteristics.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a high-uniformity ultrathin waterborne polyurethane condom is characterized by comprising the following specific steps:
s1: the aqueous polyurethane emulsion is prepared to have the solid content of 15 to 30 percent and the viscosity of 15 to 30mPa.S;
s2: cleaning a mold: cleaning the glass mold with a cleaning solution, rinsing with deionized water, and drying;
s3: dipping the isolated layer emulsion: immersing the mould into the separant emulsion for 3-10 seconds, slowly taking out the mould at the lifting speed of 2.0-3.0mm/s, and drying at 65-100 ℃ for 2-6min;
the isolation layer emulsion is a compound modified aqueous polyurethane emulsion with the solid content of 3-8%, and is prepared by compounding an organic silicon modified aqueous polyurethane emulsion, a nano silicon dioxide modified polyether aqueous polyurethane emulsion, a wetting agent, a flatting agent and a defoaming agent and filtering the mixture through a 400-mesh filter screen;
s4: dipping and film forming: immersing the mould processed in the step S3 into the aqueous polyurethane emulsion prepared in the step S1 under the condition that the relative humidity is more than 80%, wherein the immersion time is 3-10 seconds, the mould is slowly taken out at the lifting speed of 2.0-3.0mm/S, then drying for 3-8min at the temperature of 65-110 ℃, and repeating the step S4 for 2-4 times to obtain an aqueous polyurethane adhesive film on the surface of the mould;
s5: edge curling: carrying out edge curling treatment on the opening end of the waterborne polyurethane adhesive film on the surface of the die;
s6: baking: putting the mould processed in the step S5 into an oven, and baking at 70-120 ℃ for 15-30 min;
s7: dipping a release agent: immersing the mould treated in the step S6 into a special isolation release agent with the solid content of 1-8%, taking out and drying for 6-15min at the temperature of 80-110 ℃;
s8: demoulding: demolding the mold treated in the step S7 by adopting a brush roller or a rubber roller to obtain a semi-product of the waterborne polyurethane condom;
s9: electric detection: and (5) performing high-voltage dry electrical inspection on the semi-finished product of the waterborne polyurethane condom obtained in the step (S8) and removing defective products to obtain a qualified waterborne polyurethane condom product.
2. The preparation method according to claim 1, wherein the aqueous polyurethane emulsion in step S1 is a polyether/polyester aqueous polyurethane emulsion having high strength, low modulus and high resilience; 100% Young's modulus of 0.9-1.3 MPa, tensile strength of 45MPa or more, and permanent deformation of 5% or less.
3. The preparation method according to claim 1, wherein the cleaning solution in the step S2 is 2-10% of white liquor, 1-8% of diluted acid solution, and 1-10% of neutral cleaning solution.
4. The preparation method according to claim 1, wherein the wetting agent and the leveling agent used in the isolation layer emulsion in the step S3 are polyether-modified polysiloxane polymers, the defoaming agent used in the isolation layer emulsion is a polyether-modified polysiloxane solution, and the addition amounts of the wetting agent and the leveling agent are 0.05 to 0.2 percent.
5. The preparation method according to claim 1, wherein the isolating and releasing agent in the step S7 is one or two of a white carbon black aqueous dispersion, a modified corn starch aqueous dispersion, an ultrafine calcium carbonate aqueous dispersion and a cellulose aqueous dispersion.
6. The preparation method according to claim 1, wherein the electrically qualified aqueous polyurethane condom product is heat-sealed and packaged by adding a lubricant, wherein the lubricant is silicone oil or an aqueous lubricant.
7. The process according to any one of claims 1 to 6, wherein the mean thickness difference between 35mm at the closed end and 35mm at the open end of the condom is not more than 6.5%.
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| CN202110820183.1A CN115635620A (en) | 2021-07-20 | 2021-07-20 | Preparation method of high-uniformity ultrathin waterborne polyurethane condom |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110820183.1A CN115635620A (en) | 2021-07-20 | 2021-07-20 | Preparation method of high-uniformity ultrathin waterborne polyurethane condom |
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| CN202110820183.1A Pending CN115635620A (en) | 2021-07-20 | 2021-07-20 | Preparation method of high-uniformity ultrathin waterborne polyurethane condom |
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